Process for reutilizing waste material



Dec. 28, 1943. REICHEL 2337,928

I PROCESS FOR REUTILIZING WASTE MATERIAL Filed June 24, 1940 e V/SCOSE l E l I 736 ezyczmvz SUPPLY can OPHANf 11 sarmw/ve 5 4771 15 14 LAC Ql/El? COATED I L CfLLOPHANE PURE I so; VENT I SHREDDIE 16 16 17 and 3 n bfiflff/fjb l alf "3/ J O/L/UTE 26 62665075 's g V 4; 4 l 27 g coo/(m ''sumr 21 I ,3

ATTORNEY Patented Dec. 28, 1943 2,337,928 PRGCESS FOR REUTILIZING WASTE MATERIAL Frank H.

Sylvania Reichel, Fredericksburg,

Industrial Corporation,

Va., assignor to Fredericksburg, Va., a corporation of Virginia Application June 24, 1940, Serial No. 342,144

Claims.

This invention relates in general to a process for recovering waste materials resulting from the manufacture of articles formed from moistureproof coating composition is normally soluble in' proofed plasticized regenerated cellulose, and to correlated lmpovements designed to enable the several ingredients of such waste material to be reused in the manufacture of articles of regenerated cellulose.

l-leretofore in the manufacture of articles formed of regenerated cellulose a serious problem has arisen regarding the disposal of waste materials such as strips, scraps, trimmings and imperfect pleces which result from the manufacture of films, filaments, sheets, and tubes formed of regenerated cellulose. The amount of such waste material is generally in excess of the amount which can be converted into industrial uses of the waste, for example, in the manufac-' ture of Christmas decorations, novelties, packing material and the like. Therefore, the reuseof the waste product is essential for industrial econcmy. a v It is therefore a general object of the present invention to provide a process for the continuous recovery and systematic utilization of waste products resulting from ticles formed of regenerated cellulose.

It is a further object of the invention to provide a continuous process for the recovery from such waste of the coating compositions, softening agents and. regenerated cellulose used in the manufacture of articles formed of regenerated cellulose.

It is a specific object of the invention to utilize the waste products resulting from the manufacture of articles formed from viscose, for the manufacture of other or similar articles formed from these materials, such as softened, moisture-- proofed sheets of regenerated cellulose.

Other objects of the invention will in part be obvious and will in part appear hereinafter.

The'waste materials treated according to the present invention are those arising from the manufacture of pellicles of regenerated cellulose such, for example, as moistureproof Cellophane, which pellicles as are now commercially available generally comprise sheets and films of regenerated cellulose containing about from 8% to 10% by weight of water and from to by weight of a softening agent such, for example, as glycerine, and on both sides a moistureproof coatthe manufacture of armg normally comprising a cellulose derivative, a

plasticizer, a Wax and a wax-blending agent. The softening agent is normally soluble and miscible with water, but is insoluble in organic soland the vents of the type which dissolve the moistureproof coating. On the other hand, the moisturevolatile organic solvents which are normally nonsolvents of the softening agent. v

According to the process of the present invention, the waste materials resulting from the" manufacture of plasticized moistureproof pellicles of regenerated cellulose are comminu'ted and the comminuted material the moistureproof composition which is a nonsolvent for the softening agent thereby strip ping the coating from the softening agent is extracted and the comminuted material then dried, if desired, or reuti-' lized without drying in the manufacture of viscose or other cellulose derivatives. In the preferred embodiment of the process the regenerated cellulose thus recovered is utilized in the manufacture of pellicles, the softening agent recovered is reutilized in softening such pellicles and the moistureproof composition recoveredisreutilized in coating such softened pellicles,

The invention accordingly comprises the sev--' eral steps and the relation of one or more of such steps with respect to apparatus embodying features of construction, merits of parts which are adapted to effect such steps, all as exemplified in the following detailed disclosure, and the scope of the invention will be indicated in the claims. The regenerated cellulose utilized in the present invention may be derived from viscose or from the de-esterification of cellulose esters such as nitrocellulose or by precipitation from solutions of cellulose in inorganic or organic solvents. However, by way of illustration but not by way of limiting the invention, the present process will be described with reference to the manufacture of regenerated cellulose pellicles, from viscose.

The pellicles, before or after they are dried, are usually softened in a conventional manner, such as by passing them through baths comprising solutions of softening agents, such glycerine, glycol, diethylene glycol, and th In order to render the shaped articles water proof and/or moistureproof they may be treated or coated in a known manner, such as by means of suitable coating compositions. By way of 111115- tration, a suitable moistureproof coating composition which may be applied to such structures may comprise a lacquer base, a wax, a wax-blendtreated with a solvent for the pellicle, after which the comminuted uncoated material is treated with a solvent for the softening agent whereby each of the others,

combinations of elements and arrange like.

tion.

agent as it is being taken Cellophane sheet.

tureprooi' and/or waterproof coating compositions may be so employed, and it is intended that such compositions be included. in this inven- In a preferred embodiment of the invention,

the waste materials are described as resulting from the manufacture of shaped structures such as'sheets and films formed of regenerated cellulose,'and having present a softening agent and "bearing a moistureproof coating composition.

These waste materialsare comminuted as by shredding, chopping and the like. A batch of "such shredded waste material is then treated first with a volatile organic liquid which is a solvent for the moistureproof coating composition, but which is'a non-solvent of the softening agent, the remainder of the waste material being further treatedin acontinuous manner with a solvent for the softening agents present,

and then finally treated to recover the regenera'ted'cellulose substantially freefrom all extraneous materials. v The-waste materials which are thus recovered'are' continuously reutilized in'the manufacture and formation of new shaped structures of substantially the same character from which the waste materials were derived. 'Waste materials resulting from the formation of these new shaped structures may then be reutilized in the same. manner. Thus 'it will be seen that the process .Iisgcontinuous,

' and'may be so maintained and kept in operationfor an indefinite period of time.

By way of illustrating the invention, and for,

a more completeunderstanding ofthe nature and objects, reference should be had to the attached drawing in which the figure represents a diagram of the fiow of materials and the combination of steps in the preferred embodiment. A solution of viscose prepared in a manner known to the art is shown diagrammatically as being contained in tank M.- The viscose solution is then converted into a shaped structure, such as, a sheet of Cellophane, by extrusion and precipitation in tank II. p The sheet of Cellophane in the wet-gel state'is then washed, purified, and finally softened with a glycerine solution in softening bath l2. Supply tank It containing fresh quantities of glycerine is'usedfor introducing fresh supplies of glycerine into softening bath I! from time to time to replenish the softening up and used by the drying and conditioning the Cellophane sheet f material it is ordinarily ready for trimming, rolling, cutting and preparation for sale. After cutting the sheets, trimming the rolls,

and otherwise forming the finished product, the waste materia1 resulting therefrom is gathered together and passed into shredder or cutter l8,

wherein it is comminuted into fine particles.

A bath of the shredded waste particles is transferred to extractor l1, where a solvent for the coating composition carried by the waste material is passed into the extractor from the solvent supply tank I8. I A suitable solvent which may be. used for removing the moistureproof coating composition from the bath of shredded ,material may comprise a mixture ofapproxiformed of regenerated cellulose and therefore may be so employed and used in a process for preparing such, coating compositions, but it is also to be understood that other suitable solvents may be.used when the nature of the coating composition so permits. A solution of the pure solvent described is first used only with the initial batch of shredded waste material, such as at the beginning of a day's operation, or when the recovery process is first initiated. (After such initial treatment,the first or initial batch "of. waste material treated is treated a second time, this time preferably with a solu tion which has been used to perform a second extraction of a previously treated batch of waste material. After this second treatment, the extraction solvent which now contains about 1% solids by weight of coating composition is passed directly to the solvent extract storagetank I! by means of feed linev 20. Here, the solvent extract is held temporarily and for further disposition pending the accumulation of a sufilcient amount of successive solvent batchescontaining recovered coating composition, and such further disposition of this recovered material will be described hereinafter.) 1 The initial batch of shredded waste material is then treated a second time with 'aportion of the pure solvent, and the entire mass together with this solvent is dropped into cooker 2|. As this mixture is standing in the cooker to allow time for further extraction, of the coating composition, a new batch of waste material is shredded in shredder l6 and transferred to the new.

empty extractor IT.

The solvent from the second treatmentof the initial batch in cooker ii, and containing a large portion of extracted coating composition is now drained from the cooker 2!, through feed line 22 and passed to the second shredded batch of, waste material in extractor l1. After allowance for a suitable lapse of time to permit extraction of the coating composition, this solvent is then drained from the second batch in extractor i1 and passed to the solvent extract storage tank l9 by means of feed line 20.

A portion of pure solvent is now drawn from solvent supply tank It and this solvent, combined with the second batch of shredded waste material inextractor I1, is dropped into cooker 2! where it becomes mixed with the initial batch of extracted-waste material. At this stage there are now two batches of comminuted material in the .cooker. The solvent is then drawn from these two batches by means of supply line 22 and repassed to a third batch of shredded waste materialwhich has meanwhile been prepared and transferred to extractor IT. The two batches of waste material may now be said to be substantially free'of coating composition, but still retain a small amount of the extraction solvent.

Th process is thus repeated as far as the extraction of the coating composition is concerned, using a double extraction treatment on successive batches of shredded waste material, or until it is desired to suspend operations at the close of the day, or to shut down for repairs. At such time the final solvent extract containing the extracted coating composition is not repassed to extractor II, but is passed directly to the storage tank l9 from the cooker 2| by means of compositions is now conveyed fromcooker- 2|.to feed line 32. dryer 30 where it is gently heated to remove'the Referring now to the operations relating to remaining water and the moisture contentZ' The the extraction and reuse of the softening agent, material thus dried is then conveyed to tempobatches of extracted waste material combined rary storage bin 36 where it is used in themanin cooker 2| are first treated with steam from ufacture of viscose, or in the manufacture oi boiler 23. This steam is applied to the cooker cellulose ethers and other cellulose derivatives, in order to remove the last traces of residual solin a manner known to the art. This step com vent which may still be present as aresult of the pletes the cycle of the cellulosic material.

' extraction process. The treatment ofthe ma- After sufiicient accumulation ofthe extracted terial with steam completes the removal of the coating composition intemporary reserve tank last traces of residual solvent and the batch is l9, suflicient quantities are drawn therefrom and now considered free of such moistureprooi used as a-source ofsupply for forming [coatingand/or waterproof coating compositions as well compositions formed from regenerated cellulose.

- as the'residual solvent material, but still con- This is effected in lacquer tank l5,where suittainingthe softening and/or plastlcizing agents, able adjustment is made in the proportions of The steam and the residual solvent thus recovthe material by compensating for theamount of ered are condensed in condenser tank 24. The the coating composition present in the solvent, condensed water and residual solvent is then such as by the addition of further necessar'y'in- "passed to separator where they are allowed to 0 gredients. The lacquer thus formed is used'for separate by gravity and the substantially pure coating materials such as those formed fromresolventthus recovered is returned with the supgenerated cellulose, which may be articles simiply of pure solvent contained in supply tank l8. lar or identical in structure with those irom The water which remains as a result of this conwhich the recovered solvents are obtained. densation and separation process is drained and 25 It may be seen from the above disclosurethat discarded. a process has been provided for recovery and A this point the Shredded material aining reutilization of waste materials to form substaningdooker 2| comprises regenerated cellulose and tially the same products or similar products from a'softenln a ent, su a e y Subst which the waste materials have been obtained,

tial y n Softening agent is moved by the steam o for different products having similar charactreatment'ior by h action of the Solvent used teristics, with substantially-no loss or waste The to remove the coating co pfl fl Since the present invention provides for an outlet forv all vent material used is not a suitable solvent for types of waste material formed from regenefated h Softening agent Likewise the Steam treatcellulose except those sheets and films containing m does not tend m can? the Softening agent dyestufis and pigments, and thus results in a savover to the condenser 24 to any appreciable exm m raw materials and m t expense of tent, due to substantial differences in their reposing of the waste products, which products can sp boiling points and 1 0 pressuresby this process, be economically reutilized:

The two batches of shredded material remainsince certain changes may be e in t ing incooker 2| are now treated with a suitable above disclosure a different m t; of so for the Softening agents Such as the invention could be made without departing .ter', Whit!!! S PP by tank 211 in order to from the scope thereof, it is intended that all move the y ematter contained in the above description or This dilute aqueous glycerine solution is then Shown in the accompanying drawing shall be drained through line from cooker mm terpreted as illustrative and not in a limiting dilute glycerine supply tank 28. This solutionew" sense.

contammg the (mute i is i z g Having described my invention, what I'claim as gga 'f i fi g; 1 g ga new and desire to secure by Letters Patent is: sto age t hk 2 9. After sufllcient accumulation 0 continuous process for Pewvering and of glycerine L e extracted Softening agent, reut lizlng waste material resulting from the the extract is concentrated to between 10% and manufacture of motstiurepmof pemffles of regen' 12 1 i b ev rating the water pres erated cellulose containing a softening agent, the

% g y steps comprising extracting the waste material f team coils 33. I 32f; ma i ga i gfig: osohsltion is then with an organic solvent for the moistureproof transferred to Suppl tank '3 as a reserve for composition, which solvent is a non-solvent for y the softening agent and the regenerated cellulose,

t ife ni h g 2 32; till ntiy t rfiifi sfie ai Md Separately recovering the moisturepropf cornof regenerated cellulose or other similar material, 905mm, thereafter extracting he material with as described above. If necessary the extract'of f' the Softening agent, hi h solvent dilute giyceflne in the supply tank 23 may be is anon-solvent for the regenerated cellulose, and replenished from time to time with small quanseparately tecQl/ering the S ening agent, finally times of concentrated glycerine fr m tank |3 recovering the regenerated cellulose substantially by means of line 35. For example, the glycerine free of moistureprqqf compositions nds e g whichmay be concentrated in tank 29 to be- 5 agents, and relltillzmg the separated materials tween 10% and 12% is then mixed with a higher 111 the manufacture of d moistureproof p hc es concentration of glycerine in supply tank l3 in Of regenerated cellulose. I order'to obtain a solution of approximately 14% 2. In a continuous process for recovering and by weight of glycerine. This solution of 14% reutilizing waste material result ng from the glycerine is now of suitable concentration for manufacture of moistureproof pellicles 0f regenuse in the softening bath l2 for treatment of erated cellulose containing a softening agent, the sheets and films formed of regenerated cellusteps comprising extracting the waste material lose, with an organic solvent for the moistureproof The residual shredded waste material substancomposition, which solvent is a non-solvent for tially free of all softening agents and coating 15 the softening agent and the regenerated cellulose,

and separately recovering the moistureproof com position, thereafter extracting the material with asolvent forthe softening agent, which solvent is a non-solvent. for. theregenerated cellulose, and separately recovering the softening agent, finally recovering the regenerated cellulose substantially free of moistureproof compositions and softening agents, and reutilizing the-separated moistureproof composition and; the separated softening agent in the manufacture of said moistureproof pellicles of regenerated cellulose,

-3. In a continuous process for recovering and reutilizing waste material resulting from the manufacture of moistureproof pellicles of regenerated cellulose containing a softening agent, the steps comprising extracting the waste material with. an organic solvent for the moistureproof composition, which solvent is a non-solvent for the softening agent andthe regeneratedcellulose, and separately recovering the moistureproof composition, thereafter extracting the material with y a solvent for the softening agent,;which solvent is a non-solvent for the regenerated cellulose, and

separately recovering-the softening agent, finally recovering the regenerated cellulose substantially free ofmoistureproof compositions and softening agents, andmreutilizing the separated moisture-3' proof composition and the recovered regenerated cellulose residue in the manufacture of said mols-Y tureproof pellicles of regeneratedcellulose.

4. 111 a-continuous process forrecovering and reutiliz ingi waste material resulting from themanufacture of molstureproof pelliclesof regen-,

erated cellulose containinga softening agentpthe steps comprising extracting the waste material with an organic solvent for the moistureproof composition, which solvent is a non-solvent for the softening agentand the regenerated cellulose, and separately recovering the moisturep toof composition, thereafter extracting thematerial with a solvent for the-softening agent, which. solvent is a nonesolvent for the regenerated cellulose, and separately recovering the softening agent, finally recovering the regenerated cellulose substantially free of moistureproof compositions and softening agents and reutilizing the separated. moistureproof composition in the manufacture of said molstureproof pellicles of regenerated cellulose.

- 5. In a continuous process for recovering and reutillzing', waste material resulting from the manufacture of moistureproofpellicles of regenerated cellulose containing a water-soluble softening agent, the steps comprising extractin the waste material with an organic solvent for the moistureproof composition which solvent is a j agent comprising'water, which solvent is a non-' solvent for theregenerated cellulose, and separately recovering thesoftening agent, finally reg covering the regeneratedcellulose substantially free of moistureproor compositions and softening agents and reutilizing the separated moistureproof composition and the separated softening agentin the manufacture of said moistureproof pellicles of regenerated cellulose.j

6. In a continuous processfor recovering and reutilizing waste material resulting from the manufacture of moisturep roof pellicles of regen t erated cellulose containing a, softening agent comprising glycerol, "the steps comprising com-- minutin'g'said waste material, extracting said ated cellulose, and separately recovering the V moistureproof composition, thereafter extracting the material with a solvent for the glyceroL' which solvent is a non-solvent for the regener-i ated cellulose and separately recovering the glycerol, finally recovering the regenerated cellulose substantially free of molstureproof compositions and softening agents, and reutilizing the separated moistureproof composition and the separated softening agent in the manufacture of said moistureproof pellicles of regenerated cellulose. w i i i 7. In a continuous process for recovering and reutilizing waste material resulting from the manufacture of moistureproof pellicles of regenerated cellulose containing a softening agent, the steps comprising extracting the waste material with a solvent comprising a mixture of toluene and butyl acetate for the moistureproof composition, which solvent is a non-solvent for the softening agent and the regenerated cellulose, and separately recovering the moistureproof composition, thereafter extracting the material with a solvent for the softening agent, which solvent is a non-solvent for the regenerated cellulose and separately recovering the softening agent, finally recovering the regenerated cellulose substantially free ofmoistureproof compositions andsoftening agents, and reutilizing the separated moistureproof composition in the manufacture of said moistureproof pellicles of regenerated cellulose.

8. In a'continuous process for recovering and reutiliaing waste material resulting 'from the manufacture of moistur'eproof pellicles of regeneratedcellulose containing a softening agent, the steps. comprising comminuting said waste material, extracting said comminuted material with an organic solvent for the moistureproof composition, which solvent is a non-solvent for the softening agent and the regenerated cellulose, and separately recovering the moistureproof composition, thereafter treating said material with steam to remove residual solvent adhering to the waste material, extracting said material with a solvent for the softening agent, which solvent is a non-solvent for the regen erated cellulose, conducting said extraction at an elevated temperature insufficient to decompose the regenerated cellulose and separately recovering the softening agent, finally recovering theregenerated cellulose substantially free of moistureproof compositions and'softening agents. and reutilizing the separated materials in the manufacture of said moistureproof pellicles of regenerated cellulose.

' 9. In a continuous process for recovering and reutilizing waste material resulting from the manufacture of moistureproof pellicles of regenerated cellulose containing a softening agent, the steps comprising comminuting said waste material, extracting said comminuted material with a solvent comprising a mixture of toluene pose the regenerated regenerated cellulose, conducting said extraction at an elevated temperature insuflicient to decomcellulose and separately recovering the softening agent, finally recovering the regenerated cellulose substantially free of moistureproof compositions and softening agents, and reutilizing the separated materials in the manufacture of said moistureproof pellicles of regenerated cellulose.

10. In a continuous process for recovering and reutilizing waste material resulting from the manufacture of moistureproof pellicles of regenerated cellulose containing a softening agent, the steps comprising comminuting said waste material, extracting a batch of said comminuted material with an organic solvent for the moistureproof composition, which solvent is a non-solvent for the softening agent and the regenerated cellulose, and separately recovering the moistureproof composition, repeating said extraction of said batch of comminuted material with an organic solvent for the moistureproof composition, and thereafter treating a minuted material with the solvent small quantity of the containing a moistureproof composition second batch of com-' 20 tureproof compositions and softening agents, and

resulting from the second treatment of said first batch, separately recovering the moistureproof composition resulting from said extraction of said second batch, combining the extracted materials comprising said first and second batches, and treating said batches with steam to remove residual solvent adhering to said batches, and recovering said residual solvent resulting from said steam extraction, the steam treatment being insuflicient to decompose the regenerated cellulose and remove the softening agent, thereafter extracting said combined batches with a solvent for the softening agent, which solvent is a nonsolvent for the regenerated cellulose, conducting said extraction of the softening agent at an elevated temperature insufilcient to decompose the regenerated cellulose, and separately recovering the softening agent, finally recovering the,

regenerated cellulose substantially free of moisreutilizing the separated materials in the manu- 1 facture of said moistureproof pellicles of regenerated cellulose.

FRANK H. REICHEL. 

